EP0785814B1 - Procede d'extraction par pulverisation de liquides sous haute pression - Google Patents

Procede d'extraction par pulverisation de liquides sous haute pression Download PDF

Info

Publication number
EP0785814B1
EP0785814B1 EP95936450A EP95936450A EP0785814B1 EP 0785814 B1 EP0785814 B1 EP 0785814B1 EP 95936450 A EP95936450 A EP 95936450A EP 95936450 A EP95936450 A EP 95936450A EP 0785814 B1 EP0785814 B1 EP 0785814B1
Authority
EP
European Patent Office
Prior art keywords
extraction
zone
mixing
gas
loading
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired - Lifetime
Application number
EP95936450A
Other languages
German (de)
English (en)
Other versions
EP0785814A1 (fr
Inventor
Rudolf Eggers
Henning Wagner
Michael Schneider
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Meyer Lucas GmbH and Co
Cargill Texturizing Solutions Deutschland GmbH and Co KG
Original Assignee
Meyer Lucas GmbH and Co
Lucas Meyer GmbH and Co
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Meyer Lucas GmbH and Co, Lucas Meyer GmbH and Co filed Critical Meyer Lucas GmbH and Co
Publication of EP0785814A1 publication Critical patent/EP0785814A1/fr
Application granted granted Critical
Publication of EP0785814B1 publication Critical patent/EP0785814B1/fr
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

Links

Images

Classifications

    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
    • C07F9/00—Compounds containing elements of Groups 5 or 15 of the Periodic Table
    • C07F9/02—Phosphorus compounds
    • C07F9/06—Phosphorus compounds without P—C bonds
    • C07F9/08—Esters of oxyacids of phosphorus
    • C07F9/09—Esters of phosphoric acids
    • C07F9/10—Phosphatides, e.g. lecithin
    • C07F9/103—Extraction or purification by physical or chemical treatment of natural phosphatides; Preparation of compositions containing phosphatides of unknown structure
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D11/00—Solvent extraction
    • B01D11/02—Solvent extraction of solids
    • B01D11/0203—Solvent extraction of solids with a supercritical fluid

Definitions

  • the invention relates to a method for High pressure spray extraction of liquid solutions and suspensions in the pressure range up to 1000 bar with the help of compressed gases, such as CO2, propane, butane and mixtures thereof with and without additives of entraining agents such as: ethanol, propanol, methanol, acetone, Water, methyl ethyl ketone, comprising the mixing of Liquid and gas and the separation of substances.
  • compressed gases such as CO2
  • propane, butane and mixtures thereof with and without additives of entraining agents such as: ethanol, propanol, methanol, acetone, Water, methyl ethyl ketone
  • the setting is for extraction processes an optimal dwell time is necessary.
  • discontinuous Batch process results from the period of time Exposure to the extraction gas (DE 33 16 705 A1).
  • the method according to the invention enables Continuous guidance of the extraction gas at at the same time guaranteeing optimal dwell times of the Liquid in this gas.
  • the object of the invention is therefore a Specify high pressure spray extraction process in which in a Spraying device a constant fine dispersion of the Liquid is reached without pressurization and the optimum in a suitable extraction geometry Sets dwell time.
  • the load is not in one Mixing chamber instead. Rather, a distinction is made between one Mixing zone and a subsequent loading zone.
  • the High pressure spray extraction has the advantage that the prevailing process conditions positive on the spraying impact.
  • the viscosity it leads under pressure significantly increased solubility of the gas in the liquid to a significant reduction, so that the liquid can be broken up more easily into drops.
  • the reduction in the ascertained with increasing pressure Interfacial tension between the phases to be mixed leads to the formation of small drops (evidence: computer-aided Inclusion of two drops in supercritical carbon dioxide different pressures).
  • the mixing zone must also be designed geometrically so that the high kinetic energy of the compressed gas through an optimal exchange of impulses to smash the Liquid is used in small drops.
  • the spatial Design of the mixing zone in the spray extraction can both as a two-fluid nozzle with a highly turbulent cross or Swirl flow of the gas as well as two single nozzle directed towards each other (impact effect) will. It is also conceivable to use a static one Mixer with subsequent single-component atomization of the mixture from gas and liquid.
  • the design of the loading zone is based on that for the residence time necessary for the mass transfer.
  • relatively short Dwell times e.g. B. for the deoiling of crude lecithin a cylindrical design makes sense because of the Mass transfer before the impact of the sprayed particles the wall of the loading zone is closed.
  • watery Phases have greater transport resistances, so that the Loading zone longer dwell times without wall contact must enable, e.g. is for the separation of caffeine or Nicotine from aqueous solutions the spherical or cut off Cone shape is an advantage.
  • the absorbing phase almost with the entire feed stream must be loaded, e.g. that is, crude oil degumming, in which approx. 98% of the feed stream go into solution and the phosphatides in the Loading zone.
  • a certain particle formation can also be aimed for.
  • the gas mixture that forms is then characterized by a changed solution behavior, so that the desired substances precipitate as microcrystalline particles (example: extraction with CO 2 in an extraction zone with N 2 ).
  • Raw soy lecithin is in a process according to FIG. 1 as Use medium in the inner mixing chamber of a two-fluid nozzle a supercritical fluid under extraction conditions in Cross flow mixed and then as a drop dispersion in a cylindrical loading zone (14.3 mm inner diameter) sprayed.
  • the fluid takes Phase with dwell times from 20s to 40s as much oil from the Crude lecithin particles that almost completely deoiled are.
  • the deoiled lecithin is mechanically (cyclone) from the Separated fluid flow and falls as a valuable substance in powder form Raffinate collection container while the loaded fluid in a Extract separation stage at reduced pressures and Temperatures is regenerated.
  • compression in one Pump and temperature setting in one heat exchanger the regenerated fluid of the mixing zone in the circuit again be fed.
  • Extraction pressure 350 bar-1,000 bar (preferred: 450bar-700 bar)
  • Extraction temperature 60 ° C-150 ° C (preferred: 100 ° C-140 ° C)
  • Mass flow ratio (kg fluid / kg medium): 25-100 (preferred: 50 - 75)
  • Separation pressure 50 bar-200 bar (preferred: 100 bar-150 bar)
  • Separation temperature 20 ° C -80 ° C (preferred: 40 ° C - 60 ° C).
  • a raw soy lecithin with a phosphatide content of approx. 65% can have a residual oil content under the preferred conditions of less than 1.5% by weight.
  • the crude oil degumming in which the from the loaded Fluid phase precipitating raffinate and the extracted oil Forming valuable materials is with the same extraction and Separation conditions such as lecithin oiling carried out. Due to the high oil content of 98 that passes into the fluid phase % the mass flow ratio must accordingly be 100-300 increase. Although loading is preferred in one spherical geometry could be performed in a tubular loading zone at 700 bar and 120 ° C degumming to a phosphorus content of 78 ppm in the oil can be achieved.
  • the oil separation should be at the highest possible pressures be carried out so that the effort for the Recompression of the cycle gas is reduced. Suitable are therefore separation conditions where the gas remains supercritical.
  • the recompression of the Recycle gas can be so under supercritical conditions done that by the heat of compression Extraction temperature is reached. This allows both cooling to liquefy the gas before Recompression as well as heating up after the Save recompression.
  • the extraction zone is as an independent, the atomization downstream system components.
  • the extraction zone can be a pipe section or run as a container.
  • the pipe section is suitable for media immediately after exiting the atomizer form a free-flowing solid (e.g. lecithin).
  • a free-flowing solid e.g. lecithin.
  • Media that form liquid drops e.g. raw soybean oil
  • a solid only after a long extraction time must be placed in a container with a larger diameter (ideal: ball container), because these media create a form liquid film on the wall of a pipe run and thus the one obtained during the atomization Surface enlargement would be nullified.
  • the two-phase flow from the extraction zone is directly in a raffinate collection container, in which the raffinate can discontinue.
  • FIG. 8 A representation of the loading profile for the fluid in tubular loading zone is shown in Fig. 8, the relative fluid loading over the length of the loading zone has been shown. The individual parameters are in the Representation has been recorded and the mixing zone is marked with A and the loading zone has been designated B / C.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • Molecular Biology (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Extraction Or Liquid Replacement (AREA)

Claims (1)

  1. Procédé d'extraction de solutions et de suspensions liquides par pulvérisation à haute pression, dans la plage des valeurs de pression allant jusqu'à 1000 bars, à l'aide de gaz comprimés, comme CO2, le propane, le butane et des mélanges de ceux-ci, avec ou sans additions d'agents entraínants, comme l'éthanol, le propanol, le méthanol, l'acétone, l'eau et la méthyléthylcétone, comprenant la mixtion d'un liquide et d'un gaz et la séparation des substances, caractérisé en ce qu'on effectue la mixtion dans une zone de mélange, on effectue la séparation des substances des particules pulvérisées sortant de la zone de mélange dans une zone de chargement ou d'extraction spatialement séparée de ladite zone de mélange et on maintient pour les particules pulvérisées, un temps de séjour suffisant tout en leur assurant des trajectoires géométriquement optimisées en ce qui concerne le transfert des substances en vue du chargement du gaz comprimé avec les composants matériels séparés des particules pulvérisées, procédé dans lequel on utilise des trajectoires tubulaires dans le cas de temps de séjour courts nécessaires ou de milieux qui forment un solide apte à l'écoulement directement après la sortie de l'atomiseur, et on utilise des conteneurs de grand diamètre dans le cas de milieux qui forment des gouttelettes liquides ou qui forment un solide seulement après un temps d'extraction finalement long.
EP95936450A 1994-10-11 1995-10-06 Procede d'extraction par pulverisation de liquides sous haute pression Expired - Lifetime EP0785814B1 (fr)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
DE4436223 1994-10-11
DE4436223 1994-10-11
PCT/EP1995/003950 WO1996011043A1 (fr) 1994-10-11 1995-10-06 Procede d'extraction par pulverisation de liquides sous haute pression

Publications (2)

Publication Number Publication Date
EP0785814A1 EP0785814A1 (fr) 1997-07-30
EP0785814B1 true EP0785814B1 (fr) 1998-07-29

Family

ID=6530424

Family Applications (1)

Application Number Title Priority Date Filing Date
EP95936450A Expired - Lifetime EP0785814B1 (fr) 1994-10-11 1995-10-06 Procede d'extraction par pulverisation de liquides sous haute pression

Country Status (4)

Country Link
US (1) US5855786A (fr)
EP (1) EP0785814B1 (fr)
DE (1) DE59503012D1 (fr)
WO (1) WO1996011043A1 (fr)

Families Citing this family (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6312703B1 (en) * 1998-02-06 2001-11-06 Lecigel, Llc Compressed lecithin preparations
US6821413B1 (en) * 2000-08-31 2004-11-23 Fluidphase Technologies, Inc. Method and apparatus for continuous separation and reaction using supercritical fluid
EP1414633A4 (fr) * 2001-07-10 2005-01-26 Univ Technology Corp Dispositifs et procedes de production de particules
DE10252168B4 (de) * 2002-11-09 2007-01-11 Degussa Ag Verwendung eines Verfahrens zur selektiven Abtrennung von flüchtigen Aromastoffen aus einphasigen, flüssigen Ausgangsmaterialien mit einem Fett- und/oder Öl-Gehalt ≦20 Gew.-%
US20050170063A1 (en) * 2004-01-29 2005-08-04 Lalit Chordia Production of powder and viscous material
ITSA20050007A1 (it) * 2005-03-10 2006-09-11 Uni Di Salerno Processo per la pulizia di cilindri da stampa e/o da accoppiamento, utilizzati nell'industria grafica e nella produzione di imballaggi flessibili.
US20090071509A1 (en) * 2005-03-10 2009-03-19 Ernesto Reverchon Process for Cleaning Engraved Cylinders Used in Printing and Packaging Industry From Adhesive and/or Ink Residues
DE102005037210A1 (de) * 2005-08-06 2007-02-08 Degussa Ag Verfahren zur Extraktion von Fruchtwachsen
DE102009054280A1 (de) 2009-11-23 2011-08-04 Friedrich-Alexander-Universität Erlangen-Nürnberg, 91054 Verfahren zum Herauslösen von Öl aus einem Öl-/Wasser-/Feststoff-Gemisch, zugehörige Vorrichtung sowie Verwendung des Verfahrens
ES2670473T3 (es) 2015-12-04 2018-05-30 Evonik Degussa Gmbh Procedimiento mejorado para la extracción de sustancias aromatizantes a partir de fases líquidas grasas y/o acuosas

Family Cites Families (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE3011185A1 (de) * 1980-03-22 1981-10-01 Kali-Chemie Pharma Gmbh, 3000 Hannover Verfahren zur gewinnung von fuer physiologische zwecke direkt verwendbarem rin(paragraph)lecithin
DE3329249A1 (de) * 1983-08-12 1985-02-21 Skw Trostberg Ag, 8223 Trostberg Verfahren zur extraktion formlabiler fliessfaehiger massen
DE3536622A1 (de) * 1985-10-15 1987-04-16 Krupp Gmbh Verfahren und vorrichtung zur gewinnung fester stoffe aus fluessigen stoffgemischen
DE3919384A1 (de) * 1989-06-14 1990-12-20 Schmidt Hans W Gmbh & Co Verfahren und vorrichtung zum kontinuierlichen extrahieren
DE4010400C1 (fr) * 1990-03-31 1991-05-29 Fried. Krupp Gmbh, 4300 Essen, De
DE4021239C2 (de) * 1990-07-02 1994-10-27 Bruker Franzen Analytik Gmbh Verfahren und Vorrichtung zum Extrahieren gelöster flüchtiger Substanzen aus Flüssigkeiten in die Gasphase
US5258057A (en) * 1990-07-02 1993-11-02 Bruker-Franzen Analytik Gmbh Method and apparatus for extracting dissolved, volatile substances from liquids into the vapor phase
US5288511A (en) * 1990-08-23 1994-02-22 Liquid Carbonic Corporation Supercritical carbon dioxide decaffeination of acidified coffee

Also Published As

Publication number Publication date
US5855786A (en) 1999-01-05
WO1996011043A1 (fr) 1996-04-18
EP0785814A1 (fr) 1997-07-30
DE59503012D1 (de) 1998-09-03

Similar Documents

Publication Publication Date Title
DE2429291C2 (de) Verfahren und Vorrichtung zur chemischen und/oder physikalischen Behandlung von Fluiden
DE69222125T2 (de) Atomisierung von schweren Kohlenwasserstoffen
EP0475284B1 (fr) Procédé et dispositif pour agir sur des fluides au moyen d'une onde de choc de compression
DE69206296T2 (de) Superkritische Flüssigkeiten als Verdünnungsmittel bei der Verbrennung von flüssigen Brennstoffen und Abfällen.
EP0212391B1 (fr) Procédé et appareil pour le conditionnement et le prétraitement de graines oléagineuses et fruits oléagineux, en particulier les graines légumineuses
EP0785814B1 (fr) Procede d'extraction par pulverisation de liquides sous haute pression
DE60118983T2 (de) Verfahren zur herstellung von nano- und mikro-teilchen
EP0450378B1 (fr) Procédé et dispositif de traitement de matières ou de ces mélanges
DE3536622A1 (de) Verfahren und vorrichtung zur gewinnung fester stoffe aus fluessigen stoffgemischen
DE60022195T2 (de) Verfahren und vorrichtung zur herstellung von teilchen
EP0362525A2 (fr) Procédé et dispositif pour le brayage à froid
EP2315825A1 (fr) Rupture cellulaire de matières de départ végétales ou animales, par combinaison d'un procédé par pulvérisation et d'une décompression, pour extraction sélective et séparation de matières réutilisables intracellulaires
DE2746489C2 (de) Verfahren zum Herstellen von Mikrokapseln mit Flüssigkeits- und/oder mit Feststoff-Füllungen durch Sprühtrocknung unter Verwendung einer Dreifachdüse
DE3000206A1 (de) Verfahren und vorrichtung zur solubilisierung von kakao
DE1442866A1 (de) Verfahren zur Herstellung von Gemischen aus pulverfoermigen Feststoffen mit Wasser
DE2810045B2 (de) Verfahren und Vorrichtung zur Zerstäubungstrocknung von flüssigen oder pastösen Stoffen in durch Brennstoffverbrennung erzeugten Stoßwellen hoher Frequenz
DE10200226A1 (de) Hochdrucksprühextraktion
EP2129514A1 (fr) Procédé et dispositif de pressage
EP1717014B1 (fr) Procédé et dispositif de pressage
DE2746782C3 (de) Verfahren zur Gewinnung von Harzpulver und Zweistoffdüse zur Durchführung des Verfahrens
DE69826401T2 (de) Verfahren zur Herstellung von Salzkernen für Druckguss- und Spritzgussverfahren
EP0137214B1 (fr) Procédé d'extraction de masses fluides instables
AT513907B1 (de) Verfahren zur Anreicherung von Wertstoffen aus einem flüssigen Rohstoff
DE1241023B (de) Verfahren zur Abtrennung von festem Paraffin aus einer Paraffin-OEl-Mischung
DE4037284A1 (de) Rohrreaktor zur kontinuierlichen durchfuehrung chemischer reaktionen unter druck in fluider phase

Legal Events

Date Code Title Description
PUAI Public reference made under article 153(3) epc to a published international application that has entered the european phase

Free format text: ORIGINAL CODE: 0009012

17P Request for examination filed

Effective date: 19970423

AK Designated contracting states

Kind code of ref document: A1

Designated state(s): CH DE FR GB IT LI

GRAG Despatch of communication of intention to grant

Free format text: ORIGINAL CODE: EPIDOS AGRA

GRAG Despatch of communication of intention to grant

Free format text: ORIGINAL CODE: EPIDOS AGRA

GRAH Despatch of communication of intention to grant a patent

Free format text: ORIGINAL CODE: EPIDOS IGRA

17Q First examination report despatched

Effective date: 19971229

GRAH Despatch of communication of intention to grant a patent

Free format text: ORIGINAL CODE: EPIDOS IGRA

GRAA (expected) grant

Free format text: ORIGINAL CODE: 0009210

AK Designated contracting states

Kind code of ref document: B1

Designated state(s): CH DE FR GB IT LI

REG Reference to a national code

Ref country code: CH

Ref legal event code: EP

REF Corresponds to:

Ref document number: 59503012

Country of ref document: DE

Date of ref document: 19980903

GBT Gb: translation of ep patent filed (gb section 77(6)(a)/1977)

Effective date: 19981006

ET Fr: translation filed
PLBE No opposition filed within time limit

Free format text: ORIGINAL CODE: 0009261

STAA Information on the status of an ep patent application or granted ep patent

Free format text: STATUS: NO OPPOSITION FILED WITHIN TIME LIMIT

26N No opposition filed
PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: LI

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 19991031

Ref country code: CH

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 19991031

REG Reference to a national code

Ref country code: CH

Ref legal event code: PL

REG Reference to a national code

Ref country code: GB

Ref legal event code: IF02

REG Reference to a national code

Ref country code: FR

Ref legal event code: CD

PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: DE

Payment date: 20100929

Year of fee payment: 16

PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: GB

Payment date: 20101006

Year of fee payment: 16

Ref country code: IT

Payment date: 20101018

Year of fee payment: 16

PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: FR

Payment date: 20111103

Year of fee payment: 17

GBPC Gb: european patent ceased through non-payment of renewal fee

Effective date: 20121006

REG Reference to a national code

Ref country code: FR

Ref legal event code: ST

Effective date: 20130628

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: GB

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20121006

Ref country code: DE

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20130501

REG Reference to a national code

Ref country code: DE

Ref legal event code: R119

Ref document number: 59503012

Country of ref document: DE

Effective date: 20130501

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: IT

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20121006

Ref country code: FR

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20121031